JPH01268622A - Drug for external use - Google Patents

Abstract

PURPOSE:To obtain a drug for external use having a limited breaking strength of microcapsules with excellent usability, by blending microcapsules of a specific particle diameter having gelatin films swelled with water as films and enclosing a hydrophobic substance with a polyhydric alcohol. CONSTITUTION:The aimed substance prepared by a blending microcapsules, having gelatin swelled with water as a film material, enclosing a hydrophobic ingredient in a either form of liquid or solid and having 55-100mum particle diameter with a polyhydric alcohol as essential ingredients and controlling the breaking strength of the microcapsules after blending to 10-300g/cm<2>. The amount of the blended polyhydric alcohol in the drug for external use is 0.1-98wt.% and the amount of the blended microcapsules is 0.1-95wt.%. The above-mentioned drug for external use is not broken by mixing in producing cosmetics, medicines and quasi-drugs and can be readily broken by the palm in use without any feeling of foreign materials due to residual capsule films after breaking at all.

Description

[Detailed Description of the Invention] [Industrial Application Field] The present invention is applicable to cosmetics, pharmaceuticals, and quasi-drugs! ! The present invention relates to an external preparation characterized in that it contains microcapsules that are strong enough to not break when mixed at the time of manufacture, but to be broken by pressure from the palm of the hand at the time of use. More specifically, microcapsules with a particle size of 50 to 100 μm containing either liquid or solid hydrophobic substances, using water-swollen gelatin as a membrane material, coexist with polyhydric alcohol to form capsules. Its breaking strength is controlled at 10 to 300 g/am2, and no breakage is observed when mixing cosmetics, pharmaceuticals, quasi-drugs, etc. at the time of manufacturing. This is a condition in which when you rub your fingers or hands together to uniformly mix the capsule with the aqueous phase that is the base layer, the capsules slip through your fingers or palms and cannot be crushed. It has the advantage that it is easily destroyed, the contents leak out and mix well with the external phase, and there is no foreign body sensation due to the remaining capsule membrane after the destruction.
The present invention relates to an external preparation that is easy to use and has excellent effects in imparting gloss and moisturizing properties to the skin.

[Prior Art] Conventionally, microcapsules containing liquid oil and consisting of a gelatin wall membrane swollen with water have been used in external preparations, etc., and when attempted to be destroyed by compression with the palm of the hand, the wall membrane and inclusions are destroyed. Because it was flexible, it required extremely strong force. In addition, when rubbing the palms together, the microcapsules simply rolled on the skin surface or were buried in the pores, resulting in no destruction at all and the effect of the oil contained within could not be exerted. .

[Problems to be Solved by the Invention] As a method for improving these drawbacks, the wall film can be improved by adjusting the thickness of the wall film of the microcapsules or by incorporating fine powder such as titanium mica into the wall film. It is known to control the intensity. However, in the former method of adjusting the film thickness, the capsule must be made extremely thin in order to be easily destroyed in the palm of the hand, which may result in destruction during product manufacture. Furthermore, when microcapsules are prepared by the coacervation method in which a gelatin film is formed after dispersing oil in water, the capsule particle size is uneven, so even if the film thickness is the same, the breaking strength will vary depending on the size. Therefore, the breaking strength must be controlled from the film thickness and particle size, making the preparation extremely complicated. In addition, in the latter method of using fine powder, the transparency of the gelatin film is impaired depending on the type of fine powder, so it cannot be applied to products where the color of inclusions is important. Furthermore, when using the coacervation method, since fine powder is added to the outer phase, the amount of coacelate deposited on the surface of the oil droplet is extremely small, and most of it is discarded along with the outer aqueous phase during the washing process. This is disadvantageous in terms of cost, and even if the wall film contains fine powder, it has been impossible to improve the difference in breaking strength due to the size of the capsule.

Recently, solid or semi-solid oils have been mixed with liquid oils and encapsulated in microcapsules with a gelatin membrane, so that they do not break during product manufacturing and are easily broken by force from the palm of the hand during use. Although it has become possible to obtain microcapsules with strength, this method cannot be applied to products such as lotions that are low in viscosity and require ease of use, as the combination of solid oil is not very desirable. There has been a demand for microcapsules that contain liquid oil and have the strength to not break during product manufacturing, but to be easily broken by force from the palm of the hand during use.

As a result of intensive studies to solve this problem, the inventors of the present invention discovered that gelatin swollen with water was used as a membrane material, and microcapsules containing liquid oil were dispersed in a base containing polyhydric alcohol. The breaking strength of the capsule can be easily controlled by changing the type or composition of the polyhydric alcohol, and if this breaking strength is limited to a certain range, no breaking will occur during mixing at the time of manufacturing the external preparation. When applied to the skin, the capsules do not escape from the palm of the hand and can be easily compressed and disintegrated, and it is possible to produce a topical preparation containing transparent microcapsules that does not give the impression of a foreign body due to residual membranes. This discovery led to the completion of the present invention.

[Means for solving the problem] That is, the present invention consists of a membrane of gelatin moistened with water, encapsulates either a liquid or solid hydrophobic substance, and contains microscopic particles with a particle size of 50 to 100 μm. Contains capsules and polyhydric alcohol as essential ingredients, and the breaking strength of the microcapsules after blending is 10 to 300 g.
/cm2.

The configuration of the present invention will be described below.

The polyhydric alcohol blended into the external preparation of the present invention is a raw material generally used in cosmetics, pharmaceuticals, quasi-drugs, etc.↓
For example, diethylene glycol monoethyl ether, polyethylene glycol, propylene glycol, polypropylene glycol, 1,3-butylene glycol, glycerin, polyglycerin, penquerythritol, sorbitol, glucose, sucrose, xylitose, mannitol. etc.

The blending amount of the polyhydric alcohol according to the present invention in the external preparation is preferably within the range of 0.1 to 98% by weight.

Known methods may be used to produce gelatin membrane microcapsules according to the present invention, such as simple coacervation, complex coacervation, and other methods, but complex coacervation is generally the method used. Can be hired.

Next, the liquid hydrophobic components encapsulated in the gelatin membrane microcapsules include animal and vegetable oils, hydrocarbon oils, ester oils, silicone oils, higher fatty acids, higher alcohols,
Examples include vitamins, vitamin-like substances, and various fragrances, but in general, any fat-soluble raw material that can be applied to cosmetics, pharmaceuticals, quasi-drugs, etc. and has a liquid appearance with a melting point lower than room temperature (25°C) is sufficient. It is not limited to these.

In addition, solid hydrophobic components encapsulated in geladine membrane microcapsules include animal and vegetable oils, hydrocarbon oils, ester oils, higher fatty acids, higher alcohols, waxes, and fragrances, but are generally used in cosmetics, pharmaceuticals, and pharmaceuticals. Applicable to external products, etc., any fat-soluble raw material may be used as long as it has a melting point higher than room temperature and has a solid or semi-solid appearance, but is not limited to these.

Specifically, the liquid and solid hydrophobic components mentioned above are:
For example, avocado oil, camellia oil, tardle oil, macadamia nut oil, corn oil, mink oil, olive oil, rapeseed oil, egg yolk oil, sesame oil, persic oil, wheat germ oil,
Sasanqua oil, castor oil, linseed oil, safflower oil, cottonseed oil, eno oil, soybean oil, peanut oil, tea seed oil, kaya oil, rice bran oil, shinakiri oil, Japanese tung oil, jojoba oil, germ oil,
Liquid fats and oils such as triglycerin, glyceryl trioctanoate, glycerin triisopalmitate, cacao butter, coconut oil, horse tallow, hydrogenated coconut oil, palm oil, beef tallow, mutton tallow, hydrogenated beef tallow, palm kernel oil, pig intestines, beef bones Solid fats and oils such as fat, Japanese wax kernel oil, hydrogenated oil, beef leg fat, Japanese Japanese oak, hydrogenated castor oil, beeswax, candelilla wax, cotton wax, carnauba wax, paiberry wax, privet wax, spermaceti wax, montan wax, bran, lanolin, kapok wax, acetic acid Lanolin, liquid lanolin, sugar cane wax, lanolin fatty acid isopropyl, hexyl laurate, reduced lanolin, di-3-jopa wax, hard lanolin, shellac wax, POE lanolin alcohol ether, POE lanolin alcohol acetate,
Waxes such as POE cholesterol ether, lanolin fatty acid polyethylene glycol, POE hydrogenated lanolin alcohol ether, liquid paraffin, osichelite,
Hydrocarbons such as squalene, bristane, paraffin, montan, squalane, petrolatum, microcrystalline wax, isopropyl myristate, cetyl octoate, octyldodecyl myristate, isopropyl valmitate, butyl stearate, hexyl laurate,
myristyl myristate, decyl oleate, hexyldecyl dimethyloctanoate, cetyl lactate, myristyl lactate, lanolin acetate, isocetyl stearate, isocetyl instearate, cholesteryl 12-hydroxystearate, ethylene glycol di-2-ethylhexylate, dipentaerythritol Fatty acid ester, N-alkyl glycol monoisostearate, neopentyl glycol capriate, diisostearyl malate,
Di-2-heptylundecanoic acid glycerin, tri-2-
Trimethylolpropane ethylhexylate, trimethylolpropane triisostearate, pentaneerythritol tetra-2-ethylhexylate, glycerin tri-2-ethylhexylate, trimethylolpropane triisostearate, cetyl 2-ethylhexanoate,
2-ethylhexyl palmitate, glycerin trimyristate, tri-2-heptylundecanoic acid glyceride, castor oil fatty acid methyl ester, oleic acid oil, cetostearyl alcohol, acetoglyceride, 2-hebutylundecyl valmitate, shitubudel adipate , N-lauroyl-glutamic acid-2-octyldodecyl ester, di-2-hebutyl undecyl adipate, ethyl laurate, di-2-ethylhexyl cepatate, 2-hexyldecyl myristate, 2-hexyldecyl valmitate, Synthetic esters such as 2-hexyldecyl adipate, diisopropyl cepatate, 2-ethylhexyl succinate, ethyl acetate, butyl acetate, amyl acetate, triethyl citrate, lauric acid, myristic acid, valmitic acid, stearic acid, behenyl acid, oleic acid, 12-hydroxystearic acid,
Higher fatty acids such as undecanoic acid, tolic acid, lanolin fatty acid, isostearic acid, linoleic acid, lyluic acid, eicosapentaenoic acid, lauryl alcohol, cetyl alcohol, stearyl alcohol, behenyl alcohol, myristyl alcohol, oleyl alcohol, cetostearyl alcohol, monostearyl glycerin ether(
batyl alcohol), 2-decyltetrazosinol, lanolin alcohol, cholesterol, phytosterols, hexyldodecanol, isostearyl alcohol,
Linear and branched higher alcohols such as octyldodecanol,
Silicone oils such as methylpolysiloxane, methylphenylpolysiloxane, fatty acid-modified polysiloxane, fatty acid alcohol-modified polysiloxane, polyoxyalkylene-modified polysiloxane, retinol, retinol acetate, retinol palmitate, dehydroretinol, ergocalciphenol, cholecalciphenol tocopherol ,
Tocopherol acetate, tocopherol calcium succinate, ubiquinone, phytonadione, menaquinone, menadione, riboflavin butyrate, pyridoxine caprilate, pyridoxine divarnitate, pyridoxine civalmitate, vantothenyl alcohol, dicarboethoxybantothenic acid ethyl ester, acetyl vantothenyl ethyl ether, Bantothenyl ethyl ether, ascorbyl stearate, ascorbyl valmitate 1,
Examples include vitamins such as ascorbyl cybalmitate, vitamin-like substances such as α-lipoic acid and ferulic acid, and natural and synthetic fragrances. It is distinguished as a solid hydrophobic component.

The particle size of the microcapsules according to the present invention is 50 to 1
It is 100u.

Furthermore, the amount of the microcapsules according to the present invention incorporated in the external preparation is preferably within the range of 0.1 to 95% by weight.

Further, the weight ratio of the hydrophobic substance forming the capsule to the gelatin film is selected within the range of 1:0.01 to 1:10. Weight ratio of gelatin to hydrophobic component is 1:0.0
If it is smaller than 1, the strength of the capsule coating will decrease significantly,
It is not suitable for practical use because capsule destruction occurs during product manufacturing. Moreover, if the weight ratio is greater than 1:10, the amount of wall membrane in the capsule increases, and the wall membrane may remain after destruction, causing a foreign body sensation to the skin, which is not preferable.

By allowing it to coexist with the polyhydric alcohol, the breaking strength of the microcapsules can be controlled to 2 to 2000 g/cm" by the compression load measured by a creep meter.
From the perspective of formulation into external preparations, the breaking strength of the capsule in the present invention is preferably within the range of 10 to 300 g/c+++''.If the breaking strength of the capsule is lower than 10 g/cII12, there is a possibility that the capsule will break at the time of product manufacture. There is,
If the weight is higher than 300 g/cm2, it is difficult to destroy the capsules when applied to the skin, and the capsules simply roll on the skin surface, which is undesirable because the feeling of use is significantly reduced.

The breaking strength measuring instrument used by the present inventors here was specifically a creep meter Leonar model RE-3305 (manufactured by Yamaden Co., Ltd.), and the measuring method was to 8+++m with the capsule attached to the measuring device
It was compressed with a φ terralon cylindrical rod under a load of 1 g per second, and the amount of load at the time of collapse was converted to 1 am2 to obtain the breaking strength.

The above-mentioned gelatin capsule membrane according to the present invention is in itself clean and transparent, and has sufficient impermeability to the contents contained therein.

The external preparation of the present invention refers to an external preparation for cosmetics, pharmaceuticals, quasi-drugs, etc., but when trying to break it by compression with the palm of the hand during use, it does not require strong force, and the capsule membrane remains. Since it has extremely excellent usage characteristics of not causing a foreign body sensation, it is particularly preferable to use it as a cosmetic product that emphasizes usage characteristics.
Microcapsules with a particle size of 00 μm are used in lotion,
When incorporated into cosmetics such as emulsions, creams, shampoos, and conditioners, cosmetics with unprecedented effects can be obtained.

[Examples] The present invention will be described in detail below with reference to Examples, but the present invention is not limited thereto.

Example 1 10 g of acid-treated gelatin and gum arabic Log were dissolved in 200 g of purified water at 60° C., 150 g of squalane was added, and the mixture was stirred with a propeller stirrer at 11,000 rpm. Furthermore, a 10% acetic acid aqueous solution was added dropwise to this dispersion to adjust the pH to 4.
3 and diluted by adding 600 g of purified water at 40°C.

Next, while stirring, cool the liquid from outside the container until the liquid temperature reaches 8℃.
Add glutaraldehyde and stir for 2 hours to harden the capsule membrane.

In this way, the obtained product was separated from the aqueous phase by a decantation method, washed repeatedly with water, and then subjected to sieving treatment to remove excess water, and the average particle size was 70.
A μm capsule was obtained.

This microcapsule was mixed with glycerin:water=0:100.
, 10:90, 20:80, 30 near 0, 40:60,
After dispersing in solutions with seven different compositions of 60:40 and 80:20 to a weight ratio of 10%, the following formulation was used to prepare a transparent gel-like lotion. A comparative evaluation was made regarding the presence or absence of destruction due to stirring and the presence or absence of a foreign body sensation when applied to the skin.

Additionally, microcapsules were taken out of the transparent gel lotion and their breaking strength was measured.

Microcapsule dispersion solution 20.0 parts Oleyl alcohol 4.0 Polyoxyethylene (20 mol) Sorbitan monolaurate
1.5 polyoxyethylene (20 mol) lauryl ether 0.5 ethanol
10.0 Sodium polyacrylate
1.0 fragrance
0.1 Preservative Appropriate amount of purified water
The remaining experiments were conducted in the following manner.

[Evaluation of the presence or absence of capsule destruction during the preparation of lotion J The presence or absence of capsule destruction in the transparent gel-like lotion prepared according to the above formulation was determined by observation using an optical microscope.

The evaluation method is 0: No destruction seen at all Δ: Slight damage is seen ×；Everything is destroyed This was done in three stages.

[Evaluation of the presence or absence of a foreign body sensation when applied to the skin] Apply a transparent gel-like lotion containing each capsule to the skin on the inner side of the forearm, and check the presence or absence of a foreign body sensation when feeling with the palm of the hand. It was expressed as a comprehensive sensory evaluation by 10 panelists. The evaluation method was as follows: O; no foreign body sensation at all; Δ; slight foreign body sensation; ×; extremely foreign body sensation.

[Removal of capsules] The transparent gel-like lotion was centrifuged at 4000 rpm, and the microcapsules floating at the top were removed.

[Method of measuring breaking strength] Using a Teflon cylindrical rod with an 8-inch diameter attached to a creep meter Leonor RE-3305 model (manufactured by Yamaden Co., Ltd.),
The capsules spread on a flat glass plate were compressed under a load of 1 g per second, and the amount of load at the time of crushing was converted to the amount per 1 cm 2 to determine the breaking strength.

(The following is a blank space) As shown in Table 1, MicroCabbil, which has a breaking strength in the range of 10 to 300 g/cm2, was more eroded by 10 in all of the evaluation items than other microcapsules.

Example 2 Microcapsules having an average particle diameter of 85 μm were prepared in the same manner as in Example 1, encapsulating liquid paraffin and using a propeller at a stirring speed of 850 rpm.

This microcapsule was mixed with propylene glycol: water = O: 100.10:90.20:80,3 (C70
, 40:60. 60:40° 80:20, after dispersing to a weight ratio of 15%, an emollient lotion was prepared by blending with the following formulation, When each sample was applied to the skin on the inside of the forearm and rubbed with the palm of the hand, the capsule did not escape easily, the capsule easily collapsed, the contents easily leaked during application, and the capsule was smooth when applied.
The moist feeling of the skin was expressed as a comprehensive sensory evaluation by a panel of 10 people.

Evaluation, 0; quite good ○: Good Δ: Normal ×: Bad It was performed in 04 stages.

Squalane 5.0 parts Vaseline 2.0 beeswax
0.5 Sorbitan sesquioleic acid ester 0.8 Polyoxyethylene (20 mol) Oleyl ether 1.2 Scent If 0, 5 Preservative Appropriate amount Microcapsule dispersion solution 20.0 Ethanol
5.0 carboxyvinyl polymer (1,B water'l'flt&)
20.0 Potassium hydroxide o, i
The remaining amount of purified water was also measured at the same time as the breaking strength of the microcapsules taken out from the emollient lotion.

(Leaving space below) *As shown in Judgment Table 2, the closer the value of (inner content leakage amount/inner content content) is to 1, the more likely it is to leak, and capsules with a breaking strength in the range of 10 to 300 g/cm2 are It was superior to other capsules in all evaluation items.

Example 3 Cream liquid paraffin: Vitamin A balmite-1~=92:8
Maita 0 Kabubil (average particle size 58 μm) prepared in the same manner as in Example 1 with a propeller stirring speed of 1150 rpu+ was mixed with propylene glycol: glycerin: water = 50:20. :3
It was dispersed in i8' liquid having a composition of 0 to give an MM ratio of 40%, and was blended with the following formulation to obtain a cream.

Also, the breaking strength of the Mike cocapsule taken out from the cream was 6! As a result, it was 112 g/cu+''.

Miso wax 2.0 parts stearyl alcohol 5.0 stearic acid
8.0 Squalane
10,0 self-emulsifying propylene glycol monostearate 3. O Polyoxyethylene cetyl ether (20EO) 1.0 Preservative, antioxidant Appropriate amount Triethanolamine 1.0 Microbuvir dispersion
20.0 Polyethylene glycol 0
．． (5t, !J ice making remainder Example 4 Shampoo dimethyl polysiloxane: liquid paraffin = 60:40
Microcapsules (average particle diameter 92 μm) prepared in the same manner as in Example 1, containing an oil content of (weight ratio) and stirring the propeller at a speed of 800 rpm, were
．． Two bottles of 3-butylene gellicol = 40: (Dispersed at 25% in a solution with a composition of 50, and blended with the following formulation to obtain a shampoo.

Furthermore, when the breaking strength of Microcabubil taken out from the shampoo was measured, it was 253 g/cIi2.

AES-Na 18.0
part lauric acid jetanolamide 4.0 micro force dispersion iff 12, 0 preservatives, pigments, fragrances appropriate amount purified water
Remaining Example 5 Rinse squalane: Vitamin E contains oil at a ratio of 95:5 (weight ratio), and the propeller stirring speed is 1050.
Microcapsules (average particle size 63 μm) prepared in the same manner as in Example 1 were mixed with procohol: polyethylene glycol: water = 45:5.
A rinse was obtained by dispersing it in a solution with a composition of 40% and blending it according to the following formulation.

Furthermore, the breaking strength of the microcapsules taken out from the rinse was measured and found to be 211 g/cm2.

Stearyltrimethylammonium chloride 2.0 parts Cetostearyl alcohol 3.0 Glyceryl monostearate 1.5 Sodium chloride 0.2 Microparticle dispersion 18.0 Purified water
Remainder Example 6 Liquid paraffin: Vitamin C stearate = 96:4 (
Microcapsules (average particle size: 80 μm) prepared in the same manner as in Example 1, containing oil in a ratio of 7075: The hair cream oil was dispersed in a solution having a composition of 25 to a concentration of 15% and blended according to the following formulation.

Furthermore, the breaking strength of the microcapsules taken out from the hair cream oil was measured and found to be 62 g/Cm2.

Liquid paraffin 30.0 parts Microcrystalline wax 3.0 Polyoxyethylene (8 mol) Polyoxypropylene (8 mol) 2-octyl dodecyl ether 5.0 Butyl benzoate 0.1 Fragrance
0.1 oil-containing microcapsules
15.0 Purified water, remainder Cosmetic I containing Microcabuvir prepared as above
I was evaluated.

The samples used for evaluation were Examples 3 to 6 and Comparative Examples 1 to 4 below.

The evaluation method was to apply each sample to the skin on the inside of the forearm, and evaluate the difficulty of the capsule escaping when rubbed with the palm of the hand, the ease with which the capsule was crushed, the ease with which the contents leaked during application, and the smoothness during application. was expressed as a comprehensive sensory evaluation by 10 panelists.

Evaluation, 0: Pretty good O: Good △: Normal X: Bad It was performed in 04 stages.

Comparative Example 1 The same amount of propylene glycol and glycerin in the if trl in which the microcapsules of Example 3 are dispersed were replaced with water, and the mixture was blended into a cream formulation. (The breaking strength of the microcapsules taken out from the cream is 1113g/c.
It was m2. ) Comparative Example 2 The composition of the solution for dispersing the microcapsules of Example 4 was
1. 3-Butylene glycol:water" 25:75 was added to the shampoo formulation. (The breaking strength of the microcapsules taken out from Shin Vu was 498 g/
It was cm2. ) Comparative Example 3 The composition of the liquid in which the microcapsules of Example 50 are dispersed was changed to propylene glycol dipolyethylene glycol:water = 20:5 Nia 5, and this was blended into the rinse formulation. (The breaking strength of the microcapsules taken out from the rinse was 536 g/cm2.) Comparative Example 4 The same amount M of glycerin and sucrose in the solution in which the microcapsules of Example 60 are dispersed was exchanged with water, and hair cream was applied. Added to oil formulation. (The breaking strength of the microcapsules taken out from the hair cream was 1046 g/cm2.) (Leaving space below) *Judgment table - The closer the value of (amount of inclusions leakage/amount of inclusions blended) is closer to 1, the easier it is to leak. As is clear from 3, the breaking strength of the mixture of microcapsules and polyhydric alcohol is 10 to 300 g/cm.
Cosmetic products containing capsules that were controlled in the same way were rated 6 times worse than other products in all evaluation items.

[Effect of the invention 1] The external preparation of the present invention shows no breakage at all during mixing at the time of manufacturing the external preparation, is extremely stable, does not escape when used, and is easily broken in the palm of the hand, etc. Contains microcapsules that have the advantages of being able to leak substances, easily distributing oil on the skin, and not causing any foreign body sensation due to the capsule membrane remaining after destruction, making it easy to use.
It has an excellent effect in imparting lubricity and wettability to the skin.

Patent applicant: Shiseido Co., Ltd.

Claims (1)

[Claims] It consists of a membrane of gelatin swollen with water, and contains either a liquid or solid hydrophobic substance, and has a particle size of 50~
An external preparation comprising microcapsules of 100 μm and polyhydric alcohol as essential components, and having a breaking strength of 10 to 300 g/cm^2 after blending.